青海蚕豆中原花青素和左旋多巴的含量测定和品种间差异的比较

目的：建立青海蚕豆中左旋多巴和原花青素含量测定方法,测量22批样品的含量。方法：采用紫外分光光度法测量原花青素的含量,检测波长为554nm。采用HPLC法检测蚕豆中L-多巴含量：色谱柱：汉邦ODS-2（250mm×4-6mm,5μm）,流动相：甲醇-0-1mol/L冰醋酸溶液（5∶95）;流速：0-8 mL/min;测定波长：280 nm;柱温：25/3℃;进样量：20μL。结果：原花青素在75~375μg/mL范围内线性良好、L-多巴在75~375μg/mL范围内线性良好。结论：青海蚕豆中左旋多巴和原花青素含量测定方法稳定可靠。     

不同产地杭白菊多糖的含量测定

目的：建立杭白菊多糖的测定方法,比较不同产地杭白菊多糖含量的差异,为杭白菊的质量评价提供科学依据。方法：采用高锰酸钾滴定法测定浙江桐乡、江苏射阳等5个产地杭白菊多糖含量,并进行方法学考察。结果：杭白菊多糖的含量线性关系、精密度、重复性、回收率及稳定性测定结果均符合要求,不同产地杭白菊中多糖含量范围为5.27%~8.72%。结论：不同产地的杭白菊中多糖含量有一定差异,在评价的样本中,山东临沂地区杭白菊多糖含量最高。     

土茯苓中总黄酮的含量测定方法研究

目的：建立土茯苓总黄酮的含量测定方法。方法：采用70%乙醇超声提取工艺和可见分光光度法测定土茯苓中总黄酮的含量,以芦丁为对照品,在500 nm波长处测量。结果：芦丁在0.008～0.048 mg.mL-1范围内线性关系良好（r=1.000）,平均加样回收率（n=6）以芦丁计为98.34%,RSD为3.4%。结论：此方法操作简单,精密度、稳定性和重复性良好,可用于土茯苓总黄酮含量测定。     

川芎中阿魏酸含量的高效液相色谱法测定

用高效液相色谱法建立了中药川芎中阿魏酸含量的测定方法,实验结果表明：其回收率为１００．０２％,精密度为１．１６％,本文法操作简单,结果准确,可作川芎质量控制的标准。     

块根老鹳草中总鞣质的积累动态分析

通过测定块根老鹳草中总鞣质的含量,分析块根老鹳草中总鞣质的积累动态规律。方法：采用紫外分光光度法测定。结果：块根老鹳草叶中鞣质含量是花期最高,茎的鞣质含量普遍偏低;地上部分药材的鞣质含量是始果期含量最高。结论：建立了稳定、可靠的鞣质含量测定方法,块根老鹳草中鞣质的含量变化规律对于确定药材的药用部位及最佳采收期具有指导意义。     

HPLC检测三叶青块根中白藜芦醇和白藜芦醇苷含量的研究

目的：建立三叶青地下部分白藜芦醇、白藜芦醇苷以及总黄酮的提取分离和含量测定方法。方法：白藜芦醇提取分离选取溶剂为70%乙醇，白藜芦醇苷的提取分离选取溶剂为40%乙醇。含量测定采用高效液相色谱法，色谱柱选择Agilent ZORBAX SB-C18色谱柱(250 mm×4.6 mm,5μm)，流动相为甲醇-水梯度洗脱，流速为0.8 mL/min，检测波长为304 nm，柱温25℃。结果：白藜芦醇的线性关系方程为Y=113.836X+0.911 5，在0.02～2μg/mL范围内的峰面积与进样浓度线性关系良好(R²=0.997 6)。采用70%乙醇提取三叶青根茎中白藜芦醇的平均含量为0.59μg/g。白藜芦醇苷的线性关系方程为Y=52.515X-0.497 7，在0.02～2μg/mL范围内的峰面积与进样浓度线性关系良好(R²=0.994 4)。采用40%乙醇提取三叶青根茎中白藜芦醇的平均含量为1.76μg/g。结论：建立了三叶青地下部分白藜芦醇、白藜芦醇苷以及总黄酮的提取分离和含量测定方法。建立的高效液相色谱法方法简便，准确，重复性好，可应用于...     

不同产地枸杞子中多糖含量的比较研究

目的：建立枸杞子中多糖的测定方法，比较不同产地枸杞子中多糖含量的差异。方法：采用蒽酮-硫酸法测定宁夏、青海、新疆等3个产地86批次枸杞子中多糖的含量，分析差异，并进行方法学考察。结果：方法线性关系、回收率、精密度及重复性测定结果均符合要求，不同产地枸杞子中多糖含量范围为1.71%～4.56%，多糖含量高低顺序为青海>新疆>宁夏。结论：蒽酮-硫酸法可用于枸杞子多糖含量的测定，不同产地的枸杞子中多糖含量有一定差异，其中青海产地枸杞子中的多糖含量最高。     

HPLC法测定烟草不同部位、不同提取方法茄尼醇的含量

为了建立烟草不同部位、不同烟草原料中茄尼醇的含量测定方法,本文取烟草不同部位经甲醇超声提取及烟草不同提取方法的提取物,分别用高效液相色谱法测定茄尼醇的含量。结果显示,烟草茎及叶柄中茄尼醇含量极低,烤烟中的茄尼醇的含量：中部烟〉上部烟〉下部烟,烟叶档次越高茄尼醇含量越高。提取溶媒为石油醚〉丙酮〉乙醇。     

宣木瓜中多糖含量测定

目的:建立宣木瓜中多糖含量的测定方法,并测定不同采收时期的宣木瓜多糖含量。方法:在同一种植基地定期采集同一宣木瓜品种果实,以葡萄糖为对照品,采用分光光度法,以苯酚—浓硫酸为显色剂,在490 nm波长处测定吸光度,计算样品中多糖含量。结果:宣木瓜果实在生长过程中,其多糖含量在2.51%~5.08%之间,并于7月8日含量最高为5.08%。结论:本文建立的宣木瓜多糖含量的测定方法简便灵敏,精密度高,重现性好,稳定可靠;若要利用多糖含量高的宣木瓜,应适宜于7月上旬或中旬采收。     

RP-HPLC法测定酸枣仁汤中芒果苷的含量

目的：建立测定酸枣仁汤中芒果苷含量的反高效液相色谱分析方法。方法：色谱柱：WatersC18（250nm×4.6mm,5μm）;流动相：乙腈-0.1%磷酸水溶液,梯度洗脱;流速：1.0ml/min,检测波长：257nm。结果：芒果苷在0.316μg-1.264μg范围内与峰面积线性关系良好（r=0.9999）,平均加样回收率为97.64%,RSD为0.36%。结论：本方法简便、准确、可靠、重复性好,可作为酸枣仁汤中芒果苷的含量测定方法。     

盐酸黄连素对蚜虫生物活性的研究

黄连素为黄连Coptis chinensis Franch体内的主要生物碱成份。用采自贵阳花溪附近的新鲜黄连主根提取盐酸黄连素,将粗品重结晶一次后,用 HITACHI-220紫外可见分光光度计测得一次重结晶产品含盐酸黄连素91%,黄连主根中的黄连素含量为11.56%。室内生物测定结果表明,盐酸黄连素对甘蓝蚜Brevicoryne brassicae (L.)具有很强的触杀作用和较好的拒食活性。1%盐酸黄连素的乙醇溶液点滴蚜虫,96 h死亡率高达92.5%,校正死亡率为91.4%, LC₅₀值为(2.289±0.0125)g/L,回归方程Y=7.712+1.027X,相关系数r为0.958,达显著水平;1%盐酸黄连素的乙醇溶液处理叶片,24 h处理和对照叶面的蚜虫栖息率分别为20.6%和79.4%,拒食效果为74.04%, AFC₅₀值为(4.055±0.0215) g/L ,回归方程Y＝9.115+1.719X,相关系数r为0.998,达极显著水平。     

复方黄柏液的质量标准研究

本研究旨在建立复方黄柏液质量标准控制方法。实验采用薄层色谱法与高效液相色谱法对复方黄柏液中的盐酸小糪碱、绿原酸进行定性鉴别及含量测定。结果表明,复方黄柏液的盐酸小糪碱、绿原酸的薄层色谱中,在与对照品色谱相应的位置上,显相同颜色的斑点,阴性无干扰;HPLC 法测定盐酸小糪碱进样量在0.09～ 0.45 μg（r = 0.9998）范围内线性关系良好,平均加样回收率为103.4%;绿原酸进样量在0.9～4.5 μg（r = 0.9999）范围内峰面积线性关系良好,平均加样回收率为100.2%。检测出复方黄柏液中盐酸小糪碱含量平均为0.0222 mg/ml,绿原酸含量平均为0.382 mg/ml。研究证明,该方法可用于复方黄柏液的质量控制。     

Effect of berberine hydrochloride on grass carp Ctenopharyngodon idella serum bactericidal activity against Edwardsiella ictaluri

Bactericidal activity of grass carp (Ctenopharyngodon idella) serum was significantly enhanced when pre-treated with 15 mg l?1 or 3 mg l?1 of berberine hydrochloride, an effective component of several commonly used herbal medicines in aquaculture. The complement consumption experiment demonstrated that berberine hydrochloride can certainly activate fish complement system. The results of both experiments suggested that berberine hydrochloride could enhance the serum bactericidal activity in grass carp by activating the complement system and indicating the potential in the prevention or treatment of fish diseases.     

高效液相色谱法测定羊痫疯丸中盐酸小檗碱含量

目的：建立高效液相色谱法测定羊痫疯丸中盐酸小檗碱含量的方法。方法：采用Agilent ZORBAX SB-C18（250mm×4．6mm,5μm）色谱柱,流动相：乙腈-0．05mol／L磷酸二氢钠溶液（用磷酸调节pH值至3）（25：75）,流速：1．0mL／min,检测波长264nm,柱温40℃。结果：线形范围是：盐酸小檗碱0．0446～1．1150μg,r=0．9998（n=5）。平均回收率为97．25％,RSD为3．14％。结论：方法简便、快速准确,重现性好。可作为羊痫疯丸的质量控制方法。     

Study on the Interaction of β-Cyclodextrin and Berberine Hydrochloride and Its Analytical Application

The fluorescence enhancement of berberine hydrochloride (BBH) as a result of complex with β-cyclodextrin (β-CD) is investigated. The mechanism of the inclusion was studied and discussed by spectrofluoremetry and infrared spectrograms. The results showed that a 1∶1 (β-CD: BBH) complex was formed with an apparent association constant of 4.23×10² L/mol. Based on the enhancement of the fluorescent intensity of berberine hydrochloride, a new spectrofluorimetric method for the determination of BBH in the presence of β-CD was developed. The linear range was 1.00∼4.00 µg/mL with the detection limit of 5.54 ng/mL. The proposed method was successfully applied to the determination of BBH in tablets.     

小檗碱改善流感病毒性肺炎小鼠肺血管通透性的作用及机制

目的:观察小檗碱对流感病毒感染所致病毒性肺炎小鼠肺血管通透性的影响,并探讨其作用机制。方法:BALB/c小鼠108只随机分为3组,正常组、模型组、小檗碱组,25μL 50LD50病毒液滴鼻建立流感病毒感染的小鼠肺炎模型,感染后1 h,正常组和模型组予以双蒸水灌胃,小檗碱组予药物0.005 g.kg-1d-1腹腔注射;各组均给药2次/d,连续给药5 d。感染后的2 d、4 d、6 d,处死小鼠,肺组织称重以检测肺含水量;1%伊文氏兰5 mL/kg尾静脉注射检测肺血管通透性;Bicinchoninic acid(BCA)法检测肺泡灌洗液(BALF)中蛋白含量;放免法或酶免法测定肺组织中PGE2、PLA2及LT-B4含量。结果:病毒感染后,模型组肺含水量持续升高,肺血管通透性及BALF蛋白含量在感染后第4天开始明显升高,小檗碱降低了肺含水量、肺血管通透性及BALF蛋白含量(P<0.01);模型组肺组织中PGE2、PLA2、LT-B4的含量明显升高,小檗碱不同程度地抑制了PGE2、PLA2、LT-B4的表达。结论:小檗碱通过抑制流感病毒感染后肺组织中PGE2、PLA2、LT-B4的释放,降低了肺血管通透性及肺含水量,对病毒性肺炎中肺水肿的形成,起到一定的治疗作用。     

Bioanalytical chiral chromatographic technique and docking studies for enantioselective separation of meclizine hydrochloride: Application to pharmacokinetic study in rabbits

Enantiomeric resolution and molecular docking studies of meclizine hydrochloride on polysaccharide-based chiral stationary phase comprising cellulose tris(4-methylbenzoate) chiral selector (150 × 4.6 mm, 3.0 μm) were presented. The mobile phase used was acetonitrile:10mM ammonium bicarbonate (95:05, v/v). The developed technique was used to perform the enantioselective assay of meclizine hydrochloride in its marketed formulation. The elution order of meclizine hydrochloride enantiomers was determined by docking studies. Target compound was extracted from rabbit plasma using protein precipitation technique, followed by development of bioanalytical chiral separation method using the same matrix. Application of the method to determine pharmacokinetic parameters of meclizine hydrochloride enantiomers was performed using Phoenix WinNonlin 8.1 software. The results demonstrated stereoselective disposition of meclizine hydrochloride enantiomers in rabbits.     

小檗碱对甲亢性腹泻大鼠结肠及血浆中神经肽Y 含量的影响

目的:探讨小檗碱对甲状腺功能亢进(甲亢)性腹泻大鼠结肠及血浆中神经肽Y的影响,进而研究小檗碱治疗甲亢性腹泻的机制.方法:制备甲亢性腹泻大鼠模型.应用小檗碱对其干预,采用免疫组化方法测定甲亢性腹泻组、小檗碱治疗剂量组、健康组大鼠结肠神经肽Y的定位,采用酶联免疫方法检测各组大鼠血浆中神经肽Y含量的变化.结果:在结肠组织中,甲亢性腹泻组与健康对照组比较NPY表达明显增多,经小檗碱治疗后NPY表达较甲亢性腹泻组表达减少,接近健康对照组的表达.在血浆中,NPY的表达在甲亢性腹泻组与健康对照组中增多,经小檗碱治疗后NPY表达较甲亢性腹泻组表达减少,接近健康对照组的表达.结论:甲亢性腹泻大鼠结肠及血浆中NPY的表达明显增多,小檗碱治疗后NPY的表达又减少,接近健康对照组.NPY可能参与甲亢性腹泻的发生机制.     

Determination of protoberberine alkaloids in medicinal plants based on acidic potassium permanganate chemiluminescence system

A simple method was established to determine protoberberine alkaloids in Cortex Phellodendri and Rhizoma Coptidis based on an acidic potassium permanganate chemiluminescence (CL) system. The optimum conditions for the CL reaction between protoberberine alkaloids and potassium permanganate were studied in detail. Under the optimum conditions, the linear response ranges for berberine, palmatine and jatrorrhizine were 0.038–7.27, 0.031–18.1 and 0.012–3.61 μg/mL with detection limits of 0.005, 0.004 and 0.0007 μg/mL, respectively. This method was successfully applied to determine the content of protoberberine alkaloids (calculated using berberine as an index) in Cortex Phellodendri and Rhizoma Coptidis. In addition, a possible mechanism of this CL reaction was proposed on the basis of the investigation of CL, UV and fluorescent spectra of protoberberine alkaloids in acidic solution containing potassium permanganate. Copyright © 2009 John Wiley & Sons, Ltd.     

Analysis of goldenseal, Hydrastis canadensis L., and related alkaloids in urine using HPLC with UV detection

A screening method was developed to extract and detect berberine and hydrastine alkaloids from goldenseal root powder and urine samples using HPLC with UV detection. The isocratic method was developed to detect alkaloids in 5 mL of urine prior to drug screening. Urine samples were spiked with the alkaloids at varying concentrations and extracted twice with 3:1 chloroform:2-propanol (CHCl(3):2-propanol). The extracts were combined, concentrated using nitrogen gas and the residue was then reconstituted with a mobile phase of acetonitrile:buffer (32:68). A 17 min isocratic run time was performed with a flow rate of 2.0 mL/min, and UV detection at 230 nm using a C(18) (250 mm × 4.6 mm) column at room temperature. The method showed good linearity for berberine (r(2)=0.9990) and hydrastine (r(2)=0.9983) over a range of 11.80 ng/mL to 17.64 μg/mL. The LOD for berberine in urine was 12.74 ng/mL and the LOD for hydrastine in urine was 54.48 ng/mL. Urine samples were spiked with goldenseal root powder and liquid extract as part of a blinded study to determine whether berberine and hydrastine alkaloids could also be extracted in vitro from goldenseal and show a presence in urine samples. Out of the 37 blinded urine samples extracted the two spiked samples were correctly identified based on the presence or absence of berberine and hydrastine. The results demonstrated that this method will enable laboratories to test for the herbal supplement in submitted urine samples prior to drug testing, avoiding false negative results.